Fractionation



Feb. 10, 1942. J BERGMAN 2,272,261

FRACTIONATION Filed April 24, 1940 H M lzzja/ Patented Feb. 10, 1942 UNITED STATES PATENT OFFICE 2,272,261

' rnAc'rIoNA'rIoN Donald J. Bergman, Chicago, 111., assignor to Universal Oil Products Company, Chicago 111.,

a corporation of Delaware Application April 24, 1940, Serial No. 331,313

4 Claims. (Cl. 261-39) the heated vaporous stream entering the column calls for variations in the quantity of refluxing and cooling liquid supplied to the upper portion of the column if an overhead stream of constant end-boiling point is to be produced. Without compensating changes in the quantity of refluxing and cooling liquid employed, changes in the quantity of heat supplied to the column and/or in the composition of the mixture in the lower portion of the column 'will be reflected in changes in the temperature and composition of the overhead vaporous stream: Manual or automatic control of the quantity of cooling and refluxing liquid supplied to the fractionating column, in

response to minor changes in the temperature of the overhead vaporous stream leaving the col-- umn, is ordinarily employed to compensate for changing conditions within the'column before liquid, in an attempt to compensate for minor variations in the temperature of the overhead vaporous stream, as conventionally accomplished when a relatively inexpensive type of automatic control equipment, such as the present invention utilizes successfully, is employed, are quite abrupt and, in most cases, effect a too pronounced and rapid change in the opposite direction which, at

least-temporarily, upsets the smooth operation of the fractionating equipment.

To correct this difllculty, the present invention provides storage space within or adjacent the fractionating column for the refluxing and cooling liquid wherefrom the latter flows through an orifice onto the top fractionating tray and thus into contact with the vapors undergoing fractionation in the upper portion of the column. Variations in the quantity of refluxing and cooling liquid supplied to this storage space or reservoir may be accomplished by either automatic or manual control in the conventional manner they effect any substantial change in the temous stream.

I have observed that suddenchanges in the temperature at the bottom of the column are the exception rather than the rule in most fractionating operations and that they are 'apt to be of a temporary nature and not of substantial magnitude. Furthermore, due to the fact that the fractionating column ordinarily has a rather perature and composition of the overhead vapor- (e. g., in response to minor variations in the temperature of the vaporous stream leaving the fracv tionator) but due to the wide band throttling effect of the orifice abrupt changes in the rate at which refluxing and cooling liquid is supplied to the reservoir will be transmitted more gradually to the materials undergoing fractionation and abrupt changes in the temperature of these vapors is thereby prevented. This relatively simple but important improvement to conventional fractionating equipment serves to stabilize or smooth out its operation and helps to minimize the well known hunting tendency of the inexpensive automatic, control equipment. Its action maybe compared to that of relatively thick refractory walls in a heater which store up heat so large storage capacity such changes as occur in V the heat content of the vaporous stream entering the column are modified and made more gradual within the column due to commingling of the entering vapors with.the relatively large volume of vapors and liquid present in the column. Therev fore, the relatively wide temperature changes and any changes of a permanent or prolonged nature, which .are the only type than can be satisfactorily compensated for by either manual control or present inexpensive automatic control equipment, take place rather gradually,

I have also observed, on the other hand, that changes in the quantity of refluxing and cooling that abrupt changes in firing conditions are not immediately noticeable and satisfactory operation may be maintained even with control equipment of the on-and-oif type. I

\ Although, as previously indicated, the improvements provided by the invention may be utilized to advantage in the continuous fractionation of any mixture of heated vaporous or gaseous materials wherein it is desired to. produce an overhead fraction of substantially non-varying characteristics, a description of the improvement, as adapted to use with conventional fractionating equipment of the type commonly employed in oil distilling or cracking equipment, will serve to illustrate its features and advantages and various other adaptations and modifications of the apparatus illustrated will be readily apparent to those familiar with the art.

In the accompanying diagrammatic drawing Figure 1 is an elevational view, shown partially in section, of one specific form of fractionating equipment incorporating the apparatus features of the invention and with whichthe improved method of operation provided by the invention may be accomplished. Figure 2 represents a horizontal section through the fr'actionating colfixed or manually variable. gives smaller variations in flow with variations connection 3 is provided at the lower end of the column for removing condensate or bottoms therefrom and a vapor outlet connection 4 leading to suitable condensing and collecting equipment, not illustrated, is provided at the upper end of the column.

Any conventional means a such as packing, perforated trays, bubble decks and the like or any combination of such means may be employed for obtaining intimate contact between the ascending vapors and gases in the column and the descending refluxing liquid. In the particular case here illustrated, bubble decks are shown which comprise a plurality of vapor risers 5 extending through a relatively fiat tray or deck 6 and topped by bubble caps 1. A suitable level of liquid is carried on the bubble decks and the vapors passing through serrations in the skirts of the bubble caps intimately contact the liquid on the trays. The liquid passes from each tray aavaaoi form of accumulator here illustrated, refluxing liquid is discharged therefrom through conduit l4 having suitable means, such as valve 15, disposed therein ior varying the opening therethrough, the liquid passing from accumulator ll through conduit l4 and valve l5 onto the bubble tray immediately beneath the accumulator.

It is also within the scope of the invention instead of providing a valved conduit, such as H, disposed outside the Iractionating column to provide a fixed or variable orifice or weir in the lower portion of the accumulator through which liquid will flow from the latter to the bubble deck therebeneath. In any case, the means through which the flow of liquid from the accumulator into contact with the vapors undergoing fractionation is established is, in effect, an orifice or weir which may within the scope of the invention be either An orifice, since it simplest and most readily applied of the many.

possible variations. I

The size of the orifice opening, either fixed or.

'- v'ariable,is such that, with a normal level of to the next adjacent lower tray through suitable I downpipes, such as indicated at 8, which maintain the desired liquid level on each tray or deck.

The fractionating equipment so far described is conventional and, in conventional practice, refluxing liquid is directed through a line 9 containing control valve l0 into the upper portion of,

the column and is either sprayed into the vapor space in any desired manner or is introduced directly onto the tray or deck immediately beneath its point of introduction into the column.-

In the present invention this manner and means of supplying refluxing liquid to the upper portion of the column is modified and improved by providing a storage reservoir or accumulator H extending across a portion of the upper end of the column and into which the refluxing liquid from line i is intermittently introduced by opening and closing valve I0.

In the particular case here illustrated, accumulator II is formed by a portion of the cylindrical wall of the column, a relatively flat sheet or plate I! comprising a segment of a circle corresponding in diameter to the internal diameter of the column and secured along its circular edge to the cylindrical wall of the column, and a vertically extending edge plate i3 secured to member l2 along the straight edge of the latter and secured at its ends to the cylindrical wall' of the column. Many other specific forms of reservoir or accumulator may, of course, be employed-without departing fromthe scope of the invention and, when desired, the accumulator may be disposedexterior tobutadjacent the upliquid in the accumulator the rate of flow therethrough will be equivalent to the normal demand oi the iractionating column for refluxing and cooling liquid and less than the rate at which cooling and refluxing liquid is supplied to the storage reservoir when valve III is open. Thus, while valve III remains open refluxing and cooling liquid is supplied to accumulator II at a more rapid rate than that at which it is discharged from the accumulator through the orifice and the liquid level in the accumulator will rise and, by increasing the head of liquid above the orifice, increase the rate of flow therethrough and-increase the quantity of. refluxing and cooling liquid brought into contact with the vapors undergoing fractionation. On the other hand, while valve I0 remains closed no cooling and refluxing liquid is supplied to the accumulator and the level therein recedes, thereby gradually decreasing the flow through the orifice and decreasing the quantity of refluxing'and cooling liquid brought into contact with the vapors undergoing fractionation.

Valve III, which controls the flow of refluxing and cooling liquid into accumulator I i, is preferably, as in the case here illustrated, an automatic control valve of any desired type operated through-a controller indicated in the drawing at I! which functions to open and close valve ll in response to minor variations in the temperamechanism having temperature detecting means per portion of the column. With the specific 7 highly sensitive to relatively small temperature variations in order to reduce time lag in the control mechanism and maintain the temperature and composition of the fractionated vaporous stream at a relatively constant value. In the particular case here illustrated, valve III is a diaphragm control valve of the off-and-on type operated in one direction by fluid pressure transmitted to one side of the diaphra through line 20 from controller -I! and operated in the opposite direction by a spring or other loading mechanism on the opposite side of the diaphragm when in controlling the top temperature of the column pressure in line is relieved. Impulses are which obviates rapid and wide fluctuations in transmitted from a pyrometer or other suitable the top temperature due to th relatively abrupt temperature sensitive device it in line 4 to 0011- changes, obtained by conventional means. in the troller I through lin l1. Air or other suitable rate at which cooling and refluxing liquid is fluid for actuating the valve is admitted to the-lo supplied to the column. controller through line It. The controller is set Due to the number of variable factors to be. to open valve I. when the impulses transmitted considered, determination of the proper size and thereto from member l6 indicate that the temstorage capacity of-the accumulator andthe reperatureof the fractionated vaporous stream is quired size of orifice for any given fractionating slightly above that desired and to close valve column is not susceptible to accurate calculation. when the impulses transmitted to the controller For this reason, it is preferable to roughly calfrom member ll indicate that the temperature of culate th required size of the storage reservoir the fractionated vaporous stream isslightly below and the orifice, based on the average quantity that desired. 7 p of cooling and refluxing liquid required to bal When the heat supplied to the. fractionating ancetemperatures in the particular column under column is increased by an increase in the temconsideration, and to provide an accumulator of perature and/or quantity of vapors supplied ample capacity to satisfy the expected maximum thereto through line 2, an unbalanced condition requirements of the column with an orifice of is'momentarily created within the column until ample size for this maximum and with means it is reflected in a slight increase in the temfor varying the area of the latter, whereby to Denture 0f t e fractionated V p stream vary the average liquid level in the accumulator. leaving the upp r portion of the column. When For example, in designing a 5 foot diameter t s oc u the t olle w op va ve 0 and fractionating column embodying'the features of admit cooling and refluxing'liquid to accumuthe invention, wherein the normal demand for lator ll, raising the liquid level in the accumurefluxing and cooling liquid is computed to be 40 lator and increasing the fiow of liquid theregallons per minute, -I have provided. an accufrom into contact with the vapors undergoing mulatorfor the refluxing and cooling liquid which fractionation until this increased rate offlow extends over one-half the cross-sectional area corresponds to or slightly exceeds that required of the column and, assuming that the average to reestablish a temperature balance within the headof liquid in the accumulator is 1 foot, the

column. Then, as the new demand of the column for additional cooling and refluxing liquid is exceeded to the extent that the temperature I of the fractionated vaporous stream leaving the. column falls slightly below the set point of the 4 controller, the latter operates to close valve i0 and stop the supply of cooling and refluxing liquid to accumulator ll. Obviously, when the heat supplied to the fractionating column decreases, the control mechanism functions in the apparent that by providing an accumulator Iior refluxing and cooling liquid in or adjacent the 'upper portion of the tractionating column. I- provide a compensating factor for the vapor and accelerating and decelerating characteristics of the orifice discharge from the accumulator, in

.combination with the storage capacity of the accumulator, gives a wide band throttling eflect orificeopening required to deliver 40 gallons per minute of liquid from the accumulator has an area of 2.67 square inches. Since I contemplate using a relatively inexpensive and simple control mechanism of the oif-and-on type, the rate of flow of cooling and refluxing liquid into the storage reservoir will vary from zero, when valve i0 is closed, to. 200% (80 gallons per minute) of the normal demand (40 gallons per minute) of the column when valve I0 is open and closed reverse direction to stop the supply of refluxing. #5 during .equalintervals of time.' The length of and cooling liquid to the accumulator and grad-' the operating cycleof the controller from closed ually decrease the rate of flow therefrom-as the through open to closed position of valve ll will; liquid level in this zone recedes until the rate of course, vary-with varying conditions in the of fiow corresponds to the new diminished recolumn as will the -relative length of the cycle quirements of the column for refluxing and cooltime during which the valve is in an open posiing liquid. tion and a closed position. Assuming an average It will be apparent from the abov that, due cycle time of 1 minute divided into 30 second tov the sto ge capacity of the reservoir and the intervals during which the valve is open and wide band throttling efiect of the orifice, the closed, a 1 foot head of liquid in the accumulasudden surge of liquid into accumulator ii,when tor gives a storage capacity of 1.8 minutes at .valve I0 is opened, will not effect a pronounced normal demand and under normal conditions increase in the quantity of refluxing and cooling the yariation in the height of liquid is about 25% liquid brought into contact with the vapors rim of its normal height. Th'm 25% change in the dergoing fractionation and will'not immediately head of liquid above the orifice will vary the efiect a pronounced change in the temperature 11 W h r h ou appr m lv plus and of the fractionated vaporous stream leaving the minus. of the required normal fiow of 40 galcolumn. The change will be gradual andthe f ions per minute. From past experience, I berate of flow through the orifice will be accelerlieve this relatively small variation will give the ated as the level of liquid rises in the accumu- 5 results desired and the wide band throttle eflect lator. Similarly, when valve I0 is abruptly closed of the orifice is demonstrated by a comparison the rate of flow through the orifice will be g'radof this figure with the variation of the rate or ually decreased and a decelerating rate'of flow how of liquid to the accumulator which is i will occur through the orifice as the liquid level. A plus and minus of the normal demand of the in the accumulator recedes. Thus, it will be {10 column. v

particular column, provided an accumulator which will accommodate a 3 foot head of liquid and have provided an orifice which may be varied liquid storage capacity of the column and the ii in area from. zero to approximately 4 square In view of the above I have, in designing this inches.

With this ample storage capacity and ample maximum and minimum orifice opening, the normal height of the liquid in the accumulator may be varied by the operator in the fleld to obtain conditions approaching the optimum by adjusting the orifice opening; If the temperature recording instrument in the controller indicates rapid cyclic fluctuations oi considerable amplitude in the temperature of the overhead vaporous stream, the remedy is to increase the level in the storage reservoir-by decreasing the size of the variable orifice. If, on the other hand, there are long timevariations in this temperature of considerable amplitude, the remedy is to decrease the level in the storage reservoir by increasing the size of the variable orifice. The ideal condition, which may be closely approached by adjusting the orifice opening, is a minimum deviation of the temperature of the fractionated vaporous stream regardless of the length of the operating cycle of the controller and average height of liquid in the accumulator.

I claim:

1. In combination with a fractionating apparatus having a vapor inlet, an outlet for a stream 01' fractionated vapors and means within the fractionating apparatus for contacting refluxing and cooling liquid with the vapors undergoing fractionation, an accumulator providing with a conduit for supplying refluxing and cooling liquid thereto and having an orifice through which refluxing and cooling liquid may flow by gravity from the lower portion of the accumulator into contact with the vapors undergoing fractionation adjacent said vapor outlet, a temperature sensitive device disposed adjacent said vapor outlet to contact the outgoing'stream of fractionated vapors, said temperature sensitive device communicating with a controller andthe controller being operatively connected with a valve in said conduit to open and close the same in response to minor variations in the temperature of said outgoing stream of fractionated vapors.

2. In combination with a fractionating column having a vapor inlet adjacent its lower end, an outlet (or fractionated vapors adjacent its upper end and means disposed within said column for contacting the vapors undergoing fractionation therein with cooling and refluxing liquid, an accumulator for refluxing and cooling liquid disposed adJacent the upper end of said fractionating column, said accumulator being provided with a variable orlflce through which communication is established between the lower portion of said accumulator and the upper portion of said fractionating column, means including a valved conduit for supplying refluxing and cooling liquid to the accumulator, a temperature sensitive element disposed adjacent said vapor outlet to contact the outgoing stream of fractionated vapors, means for transmitting impulses resulting from minor changes in the temperature of said outgoing stream of fractionated vapors to a controller, said controller being operatively connected with said valve to open and close the same in response to said impulses.

3. In a fractionator, means for controlling the temperature thereof comprising an accumulator in said fractionator having an inlet'conduit provided with a' valve and a variable outlet orifice and atemperature sensitive device in contact with fluids in said fractionator adapted to control the opening and closing of said valve in accordance with variations in the temperature of the fluid in said fractionator.

4. In a fractionator, means for controlling the temperature thereof comprising an accumulator in said iractionator having an inlet conduit provided with a valve, said accumulator having means for conveying fluid-therefrom into contact with fluid in said fractionator and a temperature sensitive device in contact with vapors in said iractionator adapted'to control said valve.

DONALD J. BERGMAN. 

